反应详情

温度

-40 °C

A solution of 2.23 g (0.01 mol) of 4-[4-(tert-butyl)phenyl]-2-methylthiophene, 2.97 mL (0.02 mol) of TMEDA in 30 mL of ether was treated with 13 mL (0.02 mol) of 1.6M BuLi in hexane under stirring at −40° C. Then the reaction mixture was allowed to warm up to r.t. and stirred for 3 h. The reaction mixture was cooled −40° C. and treated with 1.17 g (0.01 mol) of ethyl N,N-dimethylcarbamate in 10 mL of ether. Then the reaction mixture was allowed to warm up to r.t. and was stirred overnight. Resulting mixture was treated with 10% aqueous NH4Cl, organic layer was separated, washed with 10% aqueous NH4Cl and then dried over anhydrous Na2SO4. Solvent was evaporated, the residue was washed with methanol. Yield 2.4 g (about 100%) of red oil.

1. temperatureto warm up to r.t.
2. stirringstirred for 3 h
3. temperatureThe reaction mixture was cooled −40° C.
4. temperatureto warm up to r.t.
5. stirringwas stirred overnight
6. customResulting mixture
7. customwas separated
8. washwashed with 10% aqueous NH4Cl
9. dry with materialdried over anhydrous Na2SO4
10. customSolvent was evaporated
11. washthe residue was washed with methanol